CN106497033A - A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon - Google Patents
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon Download PDFInfo
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- CN106497033A CN106497033A CN201610948513.4A CN201610948513A CN106497033A CN 106497033 A CN106497033 A CN 106497033A CN 201610948513 A CN201610948513 A CN 201610948513A CN 106497033 A CN106497033 A CN 106497033A
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- nylon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon.Which is modified by thermal field with graphene oxide as raw material, obtains modified graphene, and modified Graphene is carried out melt blending with processing aid and nylon according to component design, and gained blend composition obtains wear-resistant conductive nylon material through compression molding.The preparation method design of the present invention prepares conductive wear resistant nylon material using thermal field modified graphene using melt blending, simple in technique, be easily achieved structure regulating, has good reference for nano-carbon material/high molecular functional composite is prepared.
Description
Technical field
The invention belongs to advanced function technical field of material, and in particular to a kind of using thermal field modified graphene oxide
The method for preparing wear-resistant conductive nylon.
Background technology
Used as a kind of common engineering plastics, which has more excellent mechanical property and is widely used nylon material.Closely
Nian Lai, transport in petrochemical pipe, the application places such as electronic material substrate and sealing-in for macromolecular material electric property with
And rub resistance property proposes requirements at the higher level.
Be devoted to nylon material modified, vast research worker substantially from nylon itself graft modification, high polymer alloy with
And inorganic material filling etc. aspect be made that substantial amounts of work, define multiple effective means.With carbon fiber, CNT,
Graphene etc. for representative nano-carbon material due to itself excellent mechanics or electrical property and as conductive polymer type filler
On have comparison deep application.Go out to prepare high-strength conducting in a large number with the compound designed of nylon matrix around carbon nanomaterial
Nylon composite materials, partly come into industrialized application.Additionally, in rub resistance nylon material, putting forth effort on frictional behavior
Improve, carbon nanomaterial also has been reported that and begin to use, especially grapheme material be even more for wear-resistant macromolecule modification exist huge
Big potentiality.However, for the nylon material that electric conductivity and antiwear characteristic are taken into account is developed, open report there is no common at present.
Graphene is selected as obturator, is devoted to developing conductive wear resistant nylon material, its difficult point is to need to keep Graphene conduct
Excellent conductive filler, it is desirable to reduce the Graphene number of plies, holding graphite flake layer integrity and regulation graphenic surface group properties；
And lifting the antiwear characteristic of filling grapheme material, it is desirable to Graphene has certain number of plies, and causes Graphene and nylon base
Body has stronger combination.
Content of the invention
The present invention puts forth effort on solution Graphene as wear-resisting, conductive filler for graphenic surface functional group and lamellar structure
Requirement, be designed with atmosphere and adjust lower thermal field modified graphene, and prepare conductive wear resistant nylon using thermal field modified graphene
Method.
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, is carried out in accordance with the following steps：
(1) with graphene oxide as raw material, by carrying out heat treatment at 400-1000 DEG C under the conditions of atmosphere protection, during process
Between 1 to 4 hour, obtain heat-treatment oxidation Graphene；
(2) by heat-treatment oxidation Graphene, nylon 6 and auxiliary agent carry out melt blending, and 200-300 DEG C of blending temperature is common
Do time 5-20 minutes, obtain blend composition；
3) by blend composition compression molding, 200-300 DEG C of molding temperature, molding pressure 10-20MPa, clamp time 5-20 point
Clock, obtains conductive wear resistant nylon material.
In step (1), graphene oxide heat treatment protective atmosphere selects to use inert nitrogen gas, argon or low-level oxidation
Atmosphere；The micro-oxidizing atmosphere is the mixed gas of nitrogen and oxygen, and the volume ratio of nitrogen and oxygen is 10: (0.1-1).
0.5-10% of the thermally-denatured Graphene quality for 6 mass of nylon in step (2).
The auxiliary agent is carbon fiber and/or expanded graphite, and loading is the 0.1-5% of 6 mass of nylon.
Beneficial effects of the present invention：The present invention is based on heat effect, in the case where control climate is adjusted, realizes for Graphene top layer
Functional group's species and the regulations such as content, extent of exfoliation, it is ensured that characteristic of the thermal field modified graphene as conductive wear resistant filler, while
Improve the compatibility of Graphene and matrix.Feature of the present invention is embodied in and was based on physical field design with reference to nylon material adjuvant system
Regulation and control, the method for defining control Graphene self structure and nylon composite construction.Specifically include as follows：1. thermal field bar is adopted
Part, is adjusted by Technology for Heating Processing and atmosphere, realizes the tune with content for surface of graphene oxide official's functional group species
Control, and on the basis of keeping Graphene to complete lamellar structure as far as possible, realize the further stripping under graphene thermal field condition, reach
Arrive as excellent conductive, wear resistant filler use requirement；2. adopt melt blending, auxiliary addition agent include one-dimensional electric filler and other
Attrition resistant inorganic filler etc., realizes collaboration effect of the heterogeneous composite material system on conduction property, mechanical property and antiwear characteristic
Should, further improve material synthesis performance；3. the preparation method design adopts melt blending using thermal field modified graphene
Prepare conductive wear resistant nylon material, simple in technique, be easily achieved structure regulating, for preparing nano-carbon material/macromolecule work(
Energy composite has good reference.
Description of the drawings
Fig. 1 is thermal reduction modified graphene high resolution electron microscope photo.
Fig. 2 is thermal reduction modified graphene/nylon composite materials scanning electron micrograph.
Specific embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, is carried out in accordance with the following steps：
(1) with graphene oxide as initiation material, it is placed in ceramic crucible, is put in high-temperature experiment electric stove, is passed through
Nitrogen, and be warming up to 1000 DEG C with 5 DEG C/min and be incubated 40 minutes, 5 DEG C/min are cooled to room temperature afterwards, obtain thermal field modified
Grapheme material.Gained Graphene specific insulation is 9.30 × 10-3Ω cm, about 8 layers of the Graphene number of plies (as shown in Figure 1)；
(2) by modified for obtained thermal field Graphene and 6 melt blending of nylon, Graphene content for nylon quality 6%,
250 DEG C of melt blending temperature, obtains Graphene/nylon blending pellet；
(3) the blending granule filling obtained by enters in rectangular mould chamber, and using compression molding, molding temperature is 250 DEG C, mould
Molded pressure 15MPa, dwell time are 5 minutes, obtain the composite material sheet of 1 millimeter of thickness, obtained sheet material
Can be such as table 1.
1 thermal field modified graphene of table/nylon composite materials performance
Embodiment 2
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, is carried out in accordance with the following steps：
(1) with graphene oxide as initiation material, it is placed in ceramic crucible, is put in high-temperature experiment electric stove, is passed through
Nitrogen and oxygen mixed gas, wherein nitrogen and the volume ratio 10: 0.5 of oxygen, form micro-oxidizing atmosphere condition, and with 5 DEG C/minute
Clock is warming up to 600 DEG C and is incubated 30 minutes, and 5 DEG C/min are cooled to room temperature afterwards, obtains the modified grapheme material of thermal field.Gained
Graphene specific insulation about 2.32 × 10-2Ω cm, about 10 to 15 layers of the Graphene number of plies；
(2) by modified for obtained thermal field Graphene and 6 melt blending of nylon, Graphene content for nylon quality 5%,
250 DEG C of melt blending temperature, obtains Graphene/nylon blending pellet.
(3) the blending granule filling obtained by enters in rectangular mould chamber, and using compression molding, molding temperature is 250 DEG C, mould
Molded pressure 15MPa, dwell time are 5 minutes, obtain the composite material sheet of 1 millimeter of thickness, graphite in obtained sheet material
Alkene is dispersed in nylon, as shown in Fig. 2 its performance such as table 2.
2 thermal field modified graphene of table/nylon composite materials performance
Embodiment 3
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, is carried out in accordance with the following steps：
(1) with graphene oxide as initiation material, it is placed in ceramic crucible, is put in high-temperature experiment electric stove, is passed through
Nitrogen, and be warming up to 1000 DEG C with 5 DEG C/min and be incubated 40 minutes, 5 DEG C/min are cooled to room temperature afterwards, obtain thermal field modified
Grapheme material.Gained Graphene specific insulation is 9.30 × 10-3Ω cm, about 8 layers of the Graphene number of plies；
(2) by modified for obtained thermal field Graphene, nanometer lazurite powder and 6 melt blending of nylon, Graphene content
For the 6% of nylon quality, nanometer lazurite content of powder for nylon quality 1%, 250 DEG C of melt blending temperature obtains graphite
Alkene/nylon blending pellet；
(3) the blending granule filling obtained by enters in rectangular mould chamber, and using compression molding, molding temperature is 250 DEG C, mould
Molded pressure 15MPa, dwell time are 5 minutes, obtain the composite material sheet of 1 millimeter of thickness, obtained sheet material
Can be such as table 3.
3 thermal field modified graphene of table/nylon composite materials performance
Embodiment 4
A kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, is carried out in accordance with the following steps：
(1) with graphene oxide as initiation material, it is placed in ceramic crucible, is put in high-temperature experiment electric stove, is passed through
Nitrogen, and be warming up to 1000 DEG C with 5 DEG C/min and be incubated 40 minutes, 5 DEG C/min are cooled to room temperature afterwards, obtain thermal field modified
Grapheme material.Gained Graphene specific insulation is 9.30 × 10-3Ω cm, about 8 layers of the Graphene number of plies；
(2) by modified for obtained thermal field Graphene, nano-attapulgite and 6 melt blending of nylon, Graphene content is
The 6% of nylon quality, nano-attapulgite content for nylon quality 1%, 250 DEG C of melt blending temperature obtains Graphene/Buddhist nun
Dragon blending pellet；
(3) the blending granule filling obtained by enters in rectangular mould chamber, and using compression molding, molding temperature is 250 DEG C, mould
Molded pressure 15MPa, dwell time are 5 minutes, obtain the composite material sheet of 1 millimeter of thickness, obtained sheet material
Can be such as table 4.
4 thermal field modified graphene of table/nylon composite materials performance
Claims (4)
1. a kind of method that utilization thermal field modified graphene oxide prepares wear-resistant conductive nylon, it is characterised in that according to following step
Suddenly carry out：
(1) with graphene oxide as raw material, by carrying out heat treatment, process time 1 at 400-1000 DEG C under the conditions of atmosphere protection
To 4 hours, heat-treatment oxidation Graphene is obtained；
(2) by heat-treatment oxidation Graphene, nylon 6 and auxiliary agent carry out melt blending, and 200-300 DEG C of blending temperature, during blending
Between 5-20 minutes, obtain blend composition；
3) by blend composition compression molding, 200-300 DEG C of molding temperature, molding pressure 10-20MPa, are obtained clamp time 5-20 minute
To conductive wear resistant nylon material.
2. the method for preparing wear-resistant conductive nylon using thermal field modified graphene oxide according to claim 1, its feature exist
In in step (1), graphene oxide heat treatment protective atmosphere selects to use inert nitrogen gas, argon or micro-oxidizing atmosphere；
The micro-oxidizing atmosphere is the mixed gas of nitrogen and oxygen, and the volume ratio of nitrogen and oxygen is 10: (0.1-1).
3. the method for preparing wear-resistant conductive nylon using thermal field modified graphene oxide according to claim 1, its feature exist
In 0.5-10% of the thermally-denatured Graphene quality for 6 mass of nylon in step (2).
4. the method for preparing wear-resistant conductive nylon using thermal field modified graphene oxide according to claim 1, its feature exist
In the auxiliary agent is carbon fiber and/or expanded graphite, and loading is the 0.1-5% of 6 mass of nylon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977912A (en) * | 2017-03-20 | 2017-07-25 | 复旦大学 | A kind of preparation method of the graphene complex of nylon 6 with good electric conductivity and thermodynamic property |
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